Citation: WANG Chengyun, LI Lixia, LIN Junfeng, CHU Naiqing, XIE Tangtang. Simultaneous determination of the residues of eight isocyanates in synthesized leathers using ultra performance liquid chromatography-orbitrap high resolution mass spectrometry[J]. Chinese Journal of Chromatography, ;2016, 34(9): 888-894. doi: 10.3724/SP.J.1123.2016.04037 shu

Simultaneous determination of the residues of eight isocyanates in synthesized leathers using ultra performance liquid chromatography-orbitrap high resolution mass spectrometry

Testing and Technology Center for Industrial Products, Shenzhen Entry-Exit Inspection and Quarantine Bureau, Shenzhen 518067, China

Received Date: 25 April 2016

Fund Project: General Administration of Quality Supervision, Inspection and Quarantine (AQSIQ) Science and Technology Plan (No. 2014IK163).

An effective method of ultra performance liquid chromatography-orbitrap high resolution mass spectrometry (UPLC-Orbitrap HRMS) was established for the simultaneous determination of the residues of eight isocyanates in synthesized leathers. Residual isocyanates in synthesized leathers were ultrasonically extracted using dichloromethane as the extraction solvent and derivatized by 9-(methylaminomethyl) anthracene (MAMA) at the same time. The derivatives were concentrated and analyzed by UPLC-Orbitrap HRMS technique. The concentration of each analyte was calibrated by the external standard method. The derivatives were separated on a Hypersil GOLD column (100 mm×2.1 mm, 1.9 μm) with a gradient elution of acetonitrile and 0.1% (v/v) formic acid aqueous solution, and analyzed by Orbitrap HRMS in positive ESI mode. The qualitative analyses were carried out by the exact masses of quasi-molecular ions and the retention times. The quantitative analyses were carried out by the peak areas in extracted chromatograms. The limits of quantification (LOQs) were 0.2 μg/kg for all the eight isocyanates. The analytes were spiked in blank samples at three levels and the average recoveries varied from 85.41% to 95.53% with the relative standard deviations (RSDs) of 2.55%-6.87%. The proposed method was applied in the analysis of synthesized leather products and isophorone diisocyanate (IPDI) was detected in a real sample. The proposed method was accurate and sensitive, and applicable to the determination of the residues of isocyanates in synthesized leathers.
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